Synthesis Optimization of Guanidinium Dinitramide (GDN)

2020 ◽  
Vol 20 (11) ◽  
pp. 6855-6861
Author(s):  
Wooram Kim ◽  
Mijeong Park ◽  
Jong-Ki Jeon ◽  
Youngmin Jo

Dinitramide anion [−N(NO2)2] salt composed of resonance structure is a plausible oxidizing agents, as efficient propellant. Among them, guanidinium dinitramide (GDN) is an organic compound improving the stability against moisture, as well long term storage. An additional advantage composed guanidinium ion is the reaction efficient via the decomposed by-product during pyrognostics, maximum yield of 99%. The types of GDN (GDN-I, II, III, IV, V) were synthesized using several starting material such as guanidine acetate, chloride, carbonate, nitrate and sulfate under hydrodeprivation. In this work, the intermediates formed in these processes were closely identified and their thermal properties, and chemical structure were examined. The absorption peaks by Fourier transform infrared (FT-IR) were found guanidinium infrared frequencies (3452, 3402, 3354, 3278, 1642 cm−1) and dinitramide infrared frequencies (3208, 1570, 1492, 1416, 1337, 1179, 1000 cm−1). The activation energy of GDN samples were obtained Ea = 53.26 Kcal/mole (GDN-I), 50.94 Kcal/mole (GDN-II), 52.34 Kcal/mole (GDN-III), 62.19 Kcal/mole (GDN-IV), 55.32 Kcal/mole (GDN-V) from exothermic at over 153°C.

2008 ◽  
Vol 1 (1) ◽  
pp. 67-78 ◽  
Author(s):  
M. Hafner ◽  
M. Sulyok ◽  
R. Schuhmacher ◽  
C. Crews ◽  
R. Krska

In this paper the stability and degree of epimerisation of six major ergot alkaloids at three different temperature levels (-20 °C, +4 °C and +20 °C) over periods of 18 hours and six weeks is reported for the first time. The behaviour of ergometrine, ergocornine, ergocristine, α-ergocryptine, ergosine and ergotamine was thoroughly studied in seven solvents which are employed for the preparation of calibrants and extraction mixtures, respectively. Moreover, the stability of the ergot alkaloids was tested in different cereal extracts (rye, wheat, barley, oats) for 1, 2 and 6 days. Of the toxins tested, the ergopeptide-type toxins ergosine, ergotamine, ergocornine, α-ergocryptine and ergocristine showed similar behaviour patterns. The simple lysergic acid derivative ergometrine was more stable and showed hardly any epimerisation to ergometrinine, with the sum of both epimers remaining constant in all seven solvents. The ergopeptides tested show variable epimerisation tendencies, and were also less stable during six weeks at 20 °C. Ergosine showed the highest degree of epimerisation (43% after 6 weeks at 20 °C). In general, the order of epimerisation promotion was methanol/dichloromethane > acetonitrile/buffer > extraction mix > stabilising solution > acetonitrile >> chloroform. Long-term storage at room temperature can only be carried out in chloroform, which showed no epimerisation for all toxins even at 20 °C and also kept the sum of R and S forms constant, which indicates no formation of aci-epimers or other degradation products. Long-term storage of ergot alkaloids in acetonitrile, the most convenient solvent with respect to HPLC analysis, should be carried out at temperatures of -20 °C or below. The constant epimer ratio of all ergot alkaloids in the extraction mixture acetonitrile/ammonium carbonate buffer (200 mg/l; 92:8, v/v) during an HPLC run (18 hours) demonstrates the stability of the toxins in this extraction mixture.


Author(s):  
Sankha Bhowmick ◽  
Bharat D. Nath ◽  
John D. Biggers ◽  
Mehmet Toner

Long term preservation of mouse sperm in a desiccated state using sugars like trehalose may offer attractive economic benefits in the management of rapidly increasing transgenic mouse strains. The goal of the current study was to evaluate the protective effect of intracellular trehalose on sperm nucleus by predicting the long-term nuclear degradation kinetics of desiccated spermatozoa using an Arrhenius model whose parameters are obtained from high temperature-short time storage studies. B6D2F1 sperm isolated in an EGTA supplemented tris-HCl buffer (with or without 0.5M intracellular trehalose) were convectively dried with inert nitrogen gas in a controlled manner to moisture content >5%. The samples were then vacuum packed and stored at 22, 37, 45, 60 and 90°C for 1, 3 or 7 days. Following rehydration, the sperm sample was assayed for DNA damage using the sperm chromatin structure assay (SCSA). Results indicate significantly (p>0.05) lower DNA degradation for cells dried with intracellular trehalose at 45, 60 and 90°C for 1, 3 or 7 days compared to cells dried without trehalose. Based on a 10% increase in the index of injury, the calculated activation energy and frequency factors were 10.33 kcal/mole and 5.4×105 hr−1 respectively for cells dried in EGTA solution only. The corresponding numbers for cells dried in EGTA solution supplemented with 0.5M trehalose were 5.7 kcal/mole and 43.73 hr−1. Based on these parameters the time required for 10% DNA degradation are 279 and 759 hours for samples desiccated in plain EGTA vs. trehalose supplemented EGTA. These results indicate the beneficial effect of intracellular trehalose for the long-term storage of desiccated sperm.


2019 ◽  
Vol 974 ◽  
pp. 187-194 ◽  
Author(s):  
Nikolay V. Lyubomirskiy ◽  
Tamara A. Bakhtina ◽  
Alexander S. Bakhtin ◽  
Sergey I. Fedorkin

This paper presents the lime binding forced carbonate-hardening materials properties formation study and determins the stability of these properties during long-term storage and use under normal conditions. The tests showed these materials stability properties over time, confirming the strength and density growth of the test samples after long storage due to the calcium hydroxide recrystallization completion into calcium carbonate processes. Also, the results of the samples carbonate hardening study under natural conditions during 18 months are presented. An efficiency assessment of forced carbonate hardening as one of the methods of recycling technogenic CO2 in order to reduce its emissions in the atmosphere, and, in the result, to obtain high-quality construction materials has been made.


2018 ◽  
Vol 2018 ◽  
pp. 1-4 ◽  
Author(s):  
Eugène H. J. M. Jansen ◽  
Piet K. Beekhof

In epidemiological and nutrition research, it is very important to evaluate the stability of biomarkers as function of both storage time and temperature. In this study, the stability of folate and vitamin B12in human serum samples has been tested after long-term storage at −80°C up to 13 years. Serum samples of 16 individuals were used in this study. The concentration of folate and vitamin B12has been determined att=0and at 1, 8, and 13 years after storage at −80°C. The folate concentrations in serum samples remained stable at −80°C. The concentration of vitamin B12was decreasing during the time of the study to about 50%. The correlation of the folate and also of the vitamin B12concentrations in the stored samples compared with the starting values was still good. Therefore, although the concentration of vitamin B12decreased upon storage, reliable comparative analyses can still be performed.


2017 ◽  
Vol 81 (4) ◽  
pp. 803-811 ◽  
Author(s):  
Masahiro Ariizumi ◽  
Megumi Kubo ◽  
Akihiro Handa ◽  
Takashi Hayakawa ◽  
Kentaro Matsumiya ◽  
...  

2018 ◽  
Vol 29 (1) ◽  
pp. 94-111 ◽  
Author(s):  
Tomás Barranco ◽  
Asta Tvarijonaviciute ◽  
Damián Escribano ◽  
Fernando Tecles ◽  
José J Cerón ◽  
...  

Introduction: In this report, we aimed to examine the stability of various analytes in saliva under different storage conditions. Materials and methods: Alpha-amylase (AMY), cholinesterase (CHE), lipase (Lip), total esterase (TEA), creatine kinase (CK), aspartate aminotransferase (AST), lactate dehydrogenase (LD), lactate (Lact), adenosine deaminase (ADA), Trolox equivalent antioxidant capacity (TEAC), ferric reducing ability (FRAS), cupric reducing antioxidant capacity (CUPRAC), uric acid (UA), catalase (CAT), advanced oxidation protein products (AOPP) and hydrogen peroxide (H2O2) were colorimetrically measured in saliva obtained by passive drool from 12 healthy voluntary donors at baseline and after 3, 6, 24, 72 hours, 7 and 14 days at room temperature (RT) and 4 ºC, and after 14 days, 1, 3 and 6 months at – 20 ºC and – 80 ºC. Results: At RT, changes appeared at 6 hours for TEA and H2O2; 24 hours for Lip, CK, ADA and CUPRAC; and 72 hours for LD, Lact, FRAS, UA and AOPP. At 4 ºC changes were observed after 6 hours for TEA and H2O2; 24 hours for Lip and CUPRAC; 72 hours for CK; and 7 days for LD, FRAS and UA. At – 20 ºC changes appeared after 14 days for AST, Lip, CK and LD; and 3 months for TEA and H2O2. At – 80 ºC observed changes were after 3 months for TEA and H2O2. Conclusions: In short-term storage, the analytes were more stable at 4 ºC than at room temperature, whereas in long-term storage they were more stable at - 80 ºC than at – 20 ºC.


2018 ◽  
Vol 386 ◽  
pp. 75-79
Author(s):  
Nikolay G. Galkin ◽  
Dmitrii Tkhyarbonovich Yan ◽  
Konstantin N. Galkin ◽  
Evgeniy Anatolievich Chusovitin ◽  
Mikhail Victorovich Bozhenko

In the process of comparative studies of immersing layers of porous silicon (PS) in aqueous solutions of LiBr and Fe (NO3)3 with subsequent long-term storage up to 150 days, it is established that there exists: (1) the range of concentrations of LiBr (S/2 - S/4) and Fe (NO3)3 (0.2 M), which provide the maximum increase in the intensity of PL; (2) at low concentrations of both salts, a blue shift of the PL peaks and an increase in their intensity are observed during the long-term storage, which is associated with a decrease in the size of the NC in the PS and the influence of silicon bonds with lithium or iron ions; (3) full protection of the PS layer is observed in case of immersion in Fe (NO3)3 with a concentration of 0.7M - 0.8M.


Viruses ◽  
2021 ◽  
Vol 13 (5) ◽  
pp. 865
Author(s):  
Hans Duyvejonck ◽  
Maya Merabishvili ◽  
Mario Vaneechoutte ◽  
Steven de Soir ◽  
Rosanna Wright ◽  
...  

In Belgium, the incorporation of phages into magistral preparations for human application has been permitted since 2018. The stability of such preparations is of high importance to guarantee quality and efficacy throughout treatments. We evaluated the ability to preserve infectivity of four different phages active against three different bacterial species in five different buffer and infusion solutions commonly used in medicine and biotechnological manufacturing processes, at two different concentrations (9 and 7 log pfu/mL), stored at 4 °C. DPBS without Ca2+ and Mg2+ was found to be the best option, compared to the other solutions. Suspensions with phage concentrations of 7 log pfu/mL were unsuited as their activity dropped below the effective therapeutic dose (6–9 log pfu/mL), even after one week of storage at 4 °C. Strong variability between phages was observed, with Acinetobacter baumannii phage Acibel004 being stable in four out of five different solutions. We also studied the long term storage of lyophilized staphylococcal phage ISP, and found that the titer could be preserved during a period of almost 8 years when sucrose and trehalose were used as stabilizers. After rehydration of the lyophilized ISP phage in saline, the phage solutions remained stable at 4 °C during a period of 126 days.


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